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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.

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Designation: D 70 97

Standard Test Method for

Density of Semi-Solid Bituminous Materials (Pycnometer


Method)1
This standard is issued under the fixed designation D 70; the number immediately following the designation indicates the year of original
adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript
epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.

1. Scope
1.1 This test method covers the determination of the specific
gravity and density of semi-solid bituminous materials, asphalt
cements, and soft tar pitches by use of a pycnometer.

3.1.2 relative densitythe ratio of the mass of a given


volume of a material to the mass of the same volume of water
at the same temperature (see Note 2).

NOTE 1An alternate method for determining the density of semi-solid


and solid bituminous materials is Test Method D 3289. For materials
which are too fluid for use of this test method, use Test Method D 3142.

4. Summary of Test Method


4.1 The sample is placed in a calibrated pycnometer. The
pycnometer and sample are weighed, then the remaining
volume is filled with water. The filled pycnometer is brought to
the test temperature, and weighed. The density of the sample is
calculated from its mass and the mass of water displaced by the
sample in the filled pycnometer.

NOTE 2Relative density is also described as specific gravity.

1.2 The values in SI units are to be regarded as the standard.


1.3 This standard does not purport to address the safety
concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and
health practices and determine the applicability of regulatory
limitations prior to use.

5. Significance and Use


5.1 Values of density are used for converting volumes to
units of mass, and for correcting measured volumes from the
temperature of measurement to a standard temperature using
Practice D 4311.

2. Referenced Documents
2.1 ASTM Standards:
C 670 Practice for Preparing Precision and Bias Statements
for Test Methods for Construction Materials2
D 140 Practice for Sampling Bituminous Materials3
D 3142 Test Method for Density of Liquid Asphalts (Hydrometer Method)3
D 3289 Test Method for Density of Semi-Solid and Solid
Bituminous Materials (Nickel Crucible Method)3
D 4311 Practice for Determining Asphalt Volume Correction to a Base Temperature3
E 1 Specification for ASTM Thermometers4

6. Apparatus
6.1 Pycnometer, glass, consisting of a cylindrical or conical
vessel carefully ground to receive an accurately fitting glass
stopper 22 to 26 mm in diameter. The stopper shall be provided
with a hole 1.0 to 2.0 mm in diameter, centrally located in
reference to the vertical axis. The top surface of the stopper
shall be smooth and substantially plane, and the lower surface
shall be concave to allow all air to escape through the bore. The
height of the concave section shall be 4.0 to 18.0 mm at the
center. The stoppered pycnometer shall have a capacity of 24 to
30 mL and shall weigh not more than 40 g. Suitable pycnometers are illustrated in Fig. 1.
6.2 Water Bath, constant-temperature, capable of maintaining the temperature within 0.1C of the test temperature.
6.3 Thermometers, calibrated liquid in glass, total immersion type, of suitable range with graduations at least every
0.1C and a maximum scale error of 0.1C as prescribed in
Specification E 1. Thermometers commonly used are 63F or
63C. Any other thermometer device of equal accuracy may be
used.

3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 densitythe mass per unit volume of a material.

1
This test method is under the jurisdiction of ASTM Committee D-4 on Road
and Paving Materials and is the direct responsibility of Subcommittee D04.47 on
Miscellaneous Asphalt Tests.
Current edition approved Aug. 10, 1997. Published April 1998. Originally
published as D 70 20. Last previous edition D 70 82 (1990).
2
Annual Book of ASTM Standards, Vol 04.02.
3
Annual Book of ASTM Standards, Vol 04.03.
4
Annual Book of ASTM Standards, Vol 14.03.

Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 70 97

FIG. 1 Suitable Pycnometers and Stopper

7. Materials
7.1 WaterFreshly boiled and cooled distilled or deionized
water.

the pycnometer during weighing, quickly redry the outside of the


pycnometer (excluding the top) before recording the mass.

11. Procedure
11.1 Preparation of SampleHeat the sample with care,
stirring to prevent local overheating, until the sample has
become sufficiently fluid to pour. In no case should the
temperature be raised to more than 56C above the expected
softening point for tar, or to more than 110C above the
expected softening point for asphalt. Do not heat for more than
30 min, and avoid incorporating air bubbles into the sample.
11.2 Pour enough sample into the clean, dry, warmed
pycnometer to fill it about three fourths of its capacity. Take
precautions to keep the material from touching the sides of the
pycnometer above the final level and prevent the inclusion of
air bubbles (Note 5). Allow the pycnometer and its contents to
cool to ambient temperature for a period of not less than 40 min
and weigh with the stopper to the nearest 1 mg. Designate the
mass of the pycnometer plus sample as C.

8. Sampling
8.1 Take samples in accordance with Practice D 140. The
sample shall be free of foreign substances.
8.2 Thoroughly mix the sample before removing a representative portion for testing.
9. Preparation of Apparatus
9.1 Partially fill a 600-mL Griffin low-form beaker with
freshly boiled and cooled distilled or deionized water to a level
that will allow the top of the pycnometer to be immersed to a
depth of not less than 40 mm.
9.2 Partially immerse the beaker in the water bath to a depth
sufficient to allow the bottom of the beaker to be immersed to
a depth of not less than 100 mm, while the top of the beaker is
above the water level of the bath. Clamp the beaker in place.
9.3 Maintain the temperature of the water bath within 0.1C
of the test temperature.

NOTE 5If any air bubbles are inadvertently occluded, remove by


brushing the surface of the asphalt in the pycnometer with a high soft
flame of a bunsen burner. To avoid overheating, do not allow the flame to
remain in contact with the asphalt more than a few seconds at any one
time.

10. Calibration of Pycnometer


10.1 Thoroughly clean, dry, and weigh the pycnometer to
the nearest 1 mg. Designate this mass as A.
10.2 Remove the beaker from the water bath. Fill the
pycnometer with freshly boiled distilled or deionized water,
placing the stopper loosely in the pycnometer. Place the
pycnometer in the beaker and press the stopper firmly in place.
Return the beaker to the water bath.

11.3 Remove the beaker from the water bath. Fill the
pycnometer containing the asphalt with freshly boiled distilled
or deionized water, placing the stopper loosely in the pycnometer. Do not allow any air bubbles to remain in the pycnometer.
Place the pycnometer in the beaker and press the stopper firmly
in place. Return the beaker to the water bath.
11.4 Allow the pycnometer to remain in the water bath for
a period of not less than 30 min. Remove the pycnometer from
the bath. Dry and weigh using the same technique and timing
as that employed in 10.3. Designate this mass of pycnometer
plus sample plus water as D.

NOTE 3Calibration must be done at the test temperature. A pycnometer calibrated at one temperature cannot be used at a different temperature
without recalibration at that temperature.

10.3 Allow the pycnometer to remain in the water for a


period of not less than 30 min. Remove the pycnometer,
immediately dry the top of the stopper with one stroke of a dry
towel (Note 4), then quickly dry the remaining outside area of
the pycnometer and weigh to the nearest 1 mg. Designate the
mass of the pycnometer plus water as B.

12. Calculation
12.1 Calculate the relative density to the nearest 0.001 as
follows:
relative density 5 ~C 2 A!/@~B 2 A! 2 ~D 2 C!#

NOTE 4Do not redry the top of the stopper even even if a small
droplet of water forms as a result of expansion. If the top is dried at the
instant of removing the pycnometer from the water, the proper mass of the
contents at the test temperature will be recorded. If moisture condenses on

where:
2

(1)

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 70 97
A =
B =
C =
D =
12.2

materials has been found to be 0.0013 at 15.6C and 0.00082


at 25.0C. Therefore, results of two properly conducted tests by
the same operator on the same material should not differ by
more than the following values (see Note 6):

mass of pycnometer (plus stopper),


mass of pycnometer filled with water,
mass of pycnometer partially filled with asphalt, and
mass of pycnometer plus asphalt plus water.
Calculate density to the nearest 0.001 as follows:
Density 5 specific gravity 3 WT

Test Temperature, C
15.0
25.0

(2)

14.2 Multilaboratory PrecisionThe multilaboratory standard deviation for the relative density of semi-solid bituminous
materials has been found to be 0.0024 at 15.6C and 0.0019 at
25.0C. Therefore, results of two properly conducted tests by
two laboratories on samples of the same material should not
differ by more than the following values (see Note 6):

where:
WT = density of water at the test temperature (Note 6).
NOTE 6Density of water from CRC Handbook of Chemistry Physics:
Temperature, C
15.0
25.0

Density, kg/m3
3.7
2.3

Density of Water, kg/m3


999.1
997.0

Test Temperature, C
15.0
25.0

13. Report
13.1 Report density to the nearest 1 kg/m3 and the test
temperature.
14. Precision and Bias
14.1 Single Operator PrecisionThe single-operator standard deviation for the relative density of semi-solid bituminous

Density, kg/m3
6.8
5.4

NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 70 97
TABLE 1 Precision of Specific Gravity Data for Semi-Solid Bituminous Materials
Single-Operator
Temperature
F [C]

Degrees of
Freedom

(1S)

Multilaboratory
(D2S)

Degrees of
Freedom

(1S)

(D2S)

Asphalt

60 [15.6]
77 [25.0]

54
54

0.0011
0.00080

0.0032
0.0023

24
24

0.0018
0.0024

0.0051
0.0068

Soft tar pitch

60 [15.6]
77 [25.0]

72
72

0.0013
0.00083

0.0038
0.0023

27
27

0.0029
0.0017

0.0083
0.0048

Pooled values

60 [15.6]
77 [25.0]

114
114

0.0013
0.00082

0.0035
0.0023

51
51

0.0024
0.0019

0.0067
0.0053

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